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The title dimeric aluminium amide, [Al2(CH3)4(C6HF5N)2], contains a folded Al2N2 ring with four-coordinate Al atoms [mean Al—N = 1.9910 (14) Å and mean Al—C = 1.9452 (19) Å]. The penta­fluoro­phen­yl substituents on the N atoms adopt a trans configuration.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805017915/sj6099sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805017915/sj6099Isup2.hkl
Contains datablock I

CCDC reference: 277787

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.037
  • wR factor = 0.107
  • Data-to-parameter ratio = 16.3

checkCIF/PLATON results

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Alert level C PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.75 mm PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.88 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: P3 (Siemens, 1989); cell refinement: P3; data reduction: XDISK (Siemens, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXTL.

bis[trans-(µ2-pentafluoroanilino-κ2N:N)]bis[dimethylaluminium(III)] top
Crystal data top
[Al2(CH3)4(C6HF5N)2]Z = 2
Mr = 478.25F(000) = 480
Triclinic, P1Dx = 1.585 Mg m3
Hall symbol: -P 1Melting point: 374–390 K (dec.) K
a = 9.651 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.584 (3) ÅCell parameters from 39 reflections
c = 10.681 (3) Åθ = 7.9–12.5°
α = 82.24 (2)°µ = 0.24 mm1
β = 84.87 (2)°T = 173 K
γ = 68.06 (2)°Block, colourless
V = 1001.8 (5) Å30.75 × 0.60 × 0.60 mm
Data collection top
Rebuilt Syntex P21/Siemens P3 four-circle
diffractometer
Rint = 0.018
Radiation source: fine-focus sealed tubeθmax = 28.0°, θmin = 1.9°
Graphite monochromatorh = 1212
Wyckoff scansk = 1213
5088 measured reflectionsl = 1414
4809 independent reflections2 standard reflections every 198 reflections
4472 reflections with I > 2σ(I) intensity decay: 0.2%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0563P)2 + 0.3866P]
where P = (Fo2 + 2Fc2)/3
4809 reflections(Δ/σ)max < 0.001
295 parametersΔρmax = 0.27 e Å3
0 restraintsΔρmin = 0.25 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Al10.23105 (5)0.63965 (4)0.24040 (4)0.03044 (12)
Al20.02164 (5)0.84810 (4)0.34625 (4)0.02949 (11)
N10.19823 (13)0.80714 (13)0.32361 (11)0.0292 (2)
H10.236 (2)0.781 (2)0.394 (2)0.041 (5)*
N20.01150 (13)0.71915 (12)0.21881 (11)0.0277 (2)
H20.000 (2)0.767 (2)0.146 (2)0.043 (5)*
C10.2799 (2)0.48726 (19)0.37406 (19)0.0484 (4)
H1A0.31930.40060.33640.131 (14)*
H1B0.18960.49220.42630.099 (10)*
H1C0.35540.49230.42680.126 (13)*
C20.3481 (2)0.6351 (2)0.08299 (18)0.0476 (4)
H2A0.40190.53970.06640.117 (12)*
H2B0.42020.67890.08910.095 (10)*
H2C0.28160.68430.01380.101 (10)*
C30.0480 (2)0.7611 (2)0.51555 (16)0.0453 (4)
H3A0.15500.78650.53790.119 (12)*
H3B0.00110.79180.57690.127 (13)*
H3C0.00120.66130.51670.101 (10)*
C40.13667 (19)1.03781 (17)0.2882 (2)0.0447 (4)
H4A0.23221.06810.33670.159 (17)*
H4B0.15541.04580.19820.120 (13)*
H4C0.08051.09520.30030.125 (13)*
C110.25401 (15)0.90774 (14)0.26485 (13)0.0281 (3)
F120.12727 (11)0.93655 (11)0.07862 (9)0.0443 (2)
C120.21943 (16)0.96980 (16)0.14322 (14)0.0334 (3)
F130.24040 (15)1.12174 (14)0.03318 (12)0.0650 (4)
C130.27614 (18)1.06597 (18)0.08552 (17)0.0419 (4)
F140.42145 (15)1.19950 (14)0.09241 (15)0.0733 (4)
C140.36805 (19)1.10561 (18)0.1488 (2)0.0468 (4)
F150.48986 (14)1.08567 (14)0.33497 (14)0.0630 (3)
C150.40269 (18)1.04785 (18)0.27062 (18)0.0418 (4)
F160.38313 (12)0.89421 (12)0.44440 (9)0.0465 (2)
C160.34717 (16)0.95011 (16)0.32627 (14)0.0330 (3)
C210.07424 (15)0.63362 (14)0.22351 (12)0.0272 (3)
F220.28388 (10)0.79546 (9)0.31675 (10)0.0389 (2)
C220.21989 (15)0.67250 (14)0.27318 (13)0.0290 (3)
F230.44265 (10)0.63218 (10)0.32875 (10)0.0422 (2)
C230.30305 (16)0.59048 (15)0.27825 (14)0.0319 (3)
F240.32166 (12)0.38511 (11)0.23823 (12)0.0503 (3)
C240.24228 (17)0.46527 (15)0.23117 (15)0.0348 (3)
F250.03903 (13)0.30520 (10)0.12871 (12)0.0526 (3)
C250.09920 (18)0.42495 (15)0.17798 (15)0.0357 (3)
F260.12142 (11)0.46526 (10)0.12188 (10)0.0433 (2)
C260.01767 (16)0.50779 (15)0.17528 (14)0.0317 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Al10.0235 (2)0.0325 (2)0.0337 (2)0.00955 (16)0.00093 (16)0.00207 (17)
Al20.0265 (2)0.0326 (2)0.0324 (2)0.01465 (17)0.00489 (16)0.00647 (16)
N10.0271 (6)0.0375 (6)0.0255 (5)0.0159 (5)0.0028 (4)0.0014 (5)
N20.0252 (5)0.0307 (6)0.0283 (6)0.0121 (5)0.0005 (4)0.0018 (4)
C10.0432 (9)0.0412 (9)0.0572 (11)0.0152 (7)0.0087 (8)0.0106 (8)
C20.0347 (8)0.0610 (11)0.0454 (9)0.0162 (8)0.0122 (7)0.0133 (8)
C30.0494 (10)0.0613 (11)0.0341 (8)0.0322 (9)0.0077 (7)0.0063 (7)
C40.0345 (8)0.0322 (8)0.0677 (12)0.0135 (6)0.0059 (7)0.0078 (7)
C110.0219 (6)0.0323 (7)0.0303 (6)0.0105 (5)0.0001 (5)0.0027 (5)
F120.0390 (5)0.0631 (6)0.0363 (5)0.0266 (5)0.0146 (4)0.0082 (4)
C120.0242 (6)0.0403 (8)0.0356 (7)0.0132 (6)0.0046 (5)0.0024 (6)
F130.0613 (7)0.0748 (8)0.0549 (7)0.0318 (6)0.0141 (6)0.0349 (6)
C130.0338 (8)0.0425 (8)0.0441 (9)0.0133 (7)0.0041 (6)0.0132 (7)
F140.0642 (8)0.0606 (7)0.1045 (11)0.0436 (7)0.0017 (7)0.0168 (7)
C140.0337 (8)0.0400 (8)0.0684 (12)0.0202 (7)0.0028 (7)0.0046 (8)
F150.0529 (7)0.0720 (8)0.0853 (9)0.0422 (6)0.0072 (6)0.0205 (7)
C150.0286 (7)0.0430 (8)0.0602 (10)0.0187 (6)0.0001 (7)0.0123 (7)
F160.0462 (6)0.0673 (7)0.0334 (5)0.0270 (5)0.0091 (4)0.0075 (4)
C160.0251 (6)0.0406 (8)0.0353 (7)0.0129 (6)0.0015 (5)0.0075 (6)
C210.0263 (6)0.0293 (6)0.0265 (6)0.0113 (5)0.0034 (5)0.0002 (5)
F220.0284 (4)0.0349 (5)0.0542 (6)0.0106 (4)0.0034 (4)0.0140 (4)
C220.0271 (6)0.0284 (6)0.0313 (6)0.0096 (5)0.0036 (5)0.0025 (5)
F230.0256 (4)0.0487 (5)0.0546 (6)0.0172 (4)0.0014 (4)0.0051 (4)
C230.0237 (6)0.0364 (7)0.0355 (7)0.0121 (5)0.0040 (5)0.0014 (6)
F240.0478 (6)0.0410 (5)0.0721 (7)0.0282 (5)0.0042 (5)0.0035 (5)
C240.0354 (7)0.0319 (7)0.0412 (8)0.0179 (6)0.0078 (6)0.0023 (6)
F250.0527 (6)0.0329 (5)0.0745 (7)0.0153 (4)0.0033 (5)0.0189 (5)
C250.0395 (8)0.0265 (7)0.0412 (8)0.0114 (6)0.0037 (6)0.0047 (6)
F260.0334 (5)0.0428 (5)0.0527 (6)0.0120 (4)0.0101 (4)0.0157 (4)
C260.0278 (7)0.0324 (7)0.0329 (7)0.0093 (5)0.0001 (5)0.0032 (5)
Geometric parameters (Å, º) top
Al1—N11.9971 (14)C4—H4C0.9800
Al1—N21.9883 (14)C11—C121.383 (2)
Al2—N11.9996 (14)C11—C161.388 (2)
Al2—N21.9788 (14)F12—C121.3417 (17)
Al1—C11.9473 (19)C12—C131.379 (2)
Al1—C21.9358 (18)F13—C131.341 (2)
Al2—C31.9561 (18)C13—C141.372 (3)
Al2—C41.9417 (19)F14—C141.3348 (19)
Al1—Al22.8728 (11)C14—C151.374 (3)
N1—C111.4159 (18)F15—C151.3303 (19)
N2—C211.4306 (17)C15—C161.379 (2)
N1—H10.83 (2)F16—C161.3363 (18)
N2—H20.86 (2)C21—C221.386 (2)
C1—H1A0.9800C21—C261.389 (2)
C1—H1B0.9800F22—C221.3429 (17)
C1—H1C0.9800C22—C231.379 (2)
C2—H2A0.9800F23—C231.3382 (17)
C2—H2B0.9800C23—C241.378 (2)
C2—H2C0.9800F24—C241.3306 (17)
C3—H3A0.9800C24—C251.377 (2)
C3—H3B0.9800F25—C251.3402 (18)
C3—H3C0.9800C25—C261.376 (2)
C4—H4A0.9800F26—C261.3456 (17)
C4—H4B0.9800
N1—Al1—N285.11 (5)H3A—C3—H3B109.5
N1—Al2—N285.29 (6)Al2—C3—H3C109.5
Al1—N1—Al291.91 (6)H3A—C3—H3C109.5
Al1—N2—Al292.80 (6)H3B—C3—H3C109.5
C2—Al1—C1122.92 (9)Al2—C4—H4A109.5
C2—Al1—N2113.71 (7)Al2—C4—H4B109.5
C1—Al1—N2110.06 (7)H4A—C4—H4B109.5
C2—Al1—N1112.10 (8)Al2—C4—H4C109.5
C1—Al1—N1106.30 (8)H4A—C4—H4C109.5
C2—Al1—Al2133.32 (7)H4B—C4—H4C109.5
C1—Al1—Al2103.65 (7)C12—C11—C16115.86 (13)
N2—Al1—Al243.47 (4)C12—C11—N1122.36 (13)
N1—Al1—Al244.08 (4)C16—C11—N1121.78 (13)
C4—Al2—C3123.49 (9)F12—C12—C13118.41 (14)
C4—Al2—N2114.32 (8)F12—C12—C11119.43 (13)
C3—Al2—N2110.37 (7)C13—C12—C11122.16 (14)
C4—Al2—N1111.57 (7)F13—C13—C14119.77 (15)
C3—Al2—N1104.73 (7)F13—C13—C12119.70 (16)
C4—Al2—Al1133.45 (6)C14—C13—C12120.53 (16)
C3—Al2—Al1102.75 (7)F14—C14—C13120.03 (18)
N2—Al2—Al143.73 (4)F14—C14—C15121.07 (17)
N1—Al2—Al144.01 (4)C13—C14—C15118.90 (15)
C11—N1—Al1120.33 (9)F15—C15—C14120.24 (16)
C11—N1—Al2121.06 (10)F15—C15—C16119.87 (17)
C11—N1—H1106.1 (14)C14—C15—C16119.89 (15)
Al1—N1—H1107.4 (14)F16—C16—C15119.04 (14)
Al2—N1—H1108.9 (14)F16—C16—C11118.32 (14)
C21—N2—Al2121.42 (9)C15—C16—C11122.64 (15)
C21—N2—Al1121.30 (9)C22—C21—C26115.84 (13)
C21—N2—H2107.6 (14)C22—C21—N2122.25 (13)
Al2—N2—H2106.5 (14)C26—C21—N2121.89 (13)
Al1—N2—H2105.4 (14)F22—C22—C23118.39 (13)
Al1—C1—H1A109.5F22—C22—C21119.04 (12)
Al1—C1—H1B109.5C23—C22—C21122.57 (13)
H1A—C1—H1B109.5F23—C23—C24119.92 (13)
Al1—C1—H1C109.5F23—C23—C22120.16 (14)
H1A—C1—H1C109.5C24—C23—C22119.92 (14)
H1B—C1—H1C109.5F24—C24—C25121.06 (14)
Al1—C2—H2A109.5F24—C24—C23119.86 (14)
Al1—C2—H2B109.5C25—C24—C23119.08 (13)
H2A—C2—H2B109.5F25—C25—C26119.83 (14)
Al1—C2—H2C109.5F25—C25—C24120.20 (14)
H2A—C2—H2C109.5C26—C25—C24119.97 (14)
H2B—C2—H2C109.5F26—C26—C25118.24 (13)
Al2—C3—H3A109.5F26—C26—C21119.16 (13)
Al2—C3—H3B109.5C25—C26—C21122.59 (14)
C2—Al1—Al2—C41.26 (12)N1—C11—C12—C13178.82 (14)
C1—Al1—Al2—C4174.88 (10)F12—C12—C13—F131.1 (2)
N2—Al1—Al2—C480.24 (10)C11—C12—C13—F13179.19 (15)
N1—Al1—Al2—C475.42 (10)F12—C12—C13—C14178.49 (16)
C2—Al1—Al2—C3174.79 (10)C11—C12—C13—C141.2 (3)
C1—Al1—Al2—C31.36 (8)F13—C13—C14—F140.1 (3)
N2—Al1—Al2—C3106.24 (8)C12—C13—C14—F14179.52 (17)
N1—Al1—Al2—C398.10 (8)F13—C13—C14—C15179.64 (17)
C2—Al1—Al2—N278.98 (10)C12—C13—C14—C150.0 (3)
C1—Al1—Al2—N2104.88 (8)F14—C14—C15—F150.5 (3)
N1—Al1—Al2—N2155.66 (8)C13—C14—C15—F15179.07 (16)
C2—Al1—Al2—N176.69 (10)F14—C14—C15—C16179.38 (16)
C1—Al1—Al2—N199.46 (8)C13—C14—C15—C161.1 (3)
N2—Al1—Al2—N1155.66 (8)F15—C15—C16—F160.4 (2)
C2—Al1—N1—C112.03 (13)C14—C15—C16—F16179.42 (15)
C1—Al1—N1—C11138.90 (11)F15—C15—C16—C11179.05 (15)
N2—Al1—N1—C11111.60 (11)C14—C15—C16—C111.1 (3)
Al2—Al1—N1—C11128.14 (12)C12—C11—C16—F16179.46 (13)
C2—Al1—N1—Al2130.17 (7)N1—C11—C16—F160.5 (2)
C1—Al1—N1—Al292.96 (8)C12—C11—C16—C150.0 (2)
N2—Al1—N1—Al216.53 (5)N1—C11—C16—C15179.96 (14)
C4—Al2—N1—C113.35 (13)Al2—N2—C21—C2229.81 (17)
C3—Al2—N1—C11139.19 (12)Al1—N2—C21—C22145.80 (11)
N2—Al2—N1—C11110.97 (11)Al2—N2—C21—C26151.97 (11)
Al1—Al2—N1—C11127.58 (13)Al1—N2—C21—C2635.98 (17)
C4—Al2—N1—Al1130.92 (8)C26—C21—C22—F22177.30 (12)
C3—Al2—N1—Al193.23 (8)N2—C21—C22—F221.0 (2)
N2—Al2—N1—Al116.61 (5)C26—C21—C22—C231.8 (2)
C4—Al2—N2—C21101.99 (12)N2—C21—C22—C23179.86 (13)
C3—Al2—N2—C2142.46 (13)F22—C22—C23—F231.8 (2)
N1—Al2—N2—C21146.44 (11)C21—C22—C23—F23179.11 (13)
Al1—Al2—N2—C21129.74 (12)F22—C22—C23—C24178.21 (13)
C4—Al2—N2—Al1128.26 (7)C21—C22—C23—C240.9 (2)
C3—Al2—N2—Al187.28 (8)F23—C23—C24—F241.3 (2)
N1—Al2—N2—Al116.70 (5)C22—C23—C24—F24178.76 (13)
C2—Al1—N2—C21101.43 (12)F23—C23—C24—C25179.11 (13)
C1—Al1—N2—C2140.97 (13)C22—C23—C24—C250.9 (2)
N1—Al1—N2—C21146.55 (11)F24—C24—C25—F252.0 (2)
Al2—Al1—N2—C21129.83 (12)C23—C24—C25—F25178.33 (14)
C2—Al1—N2—Al2128.74 (8)F24—C24—C25—C26178.00 (14)
C1—Al1—N2—Al288.86 (8)C23—C24—C25—C261.6 (2)
N1—Al1—N2—Al216.72 (5)F25—C25—C26—F260.3 (2)
Al1—N1—C11—C1255.13 (17)C24—C25—C26—F26179.63 (14)
Al2—N1—C11—C1258.29 (18)F25—C25—C26—C21179.30 (14)
Al1—N1—C11—C16124.86 (13)C24—C25—C26—C210.7 (2)
Al2—N1—C11—C16121.73 (13)C22—C21—C26—F26177.93 (12)
C16—C11—C12—F12178.52 (13)N2—C21—C26—F260.4 (2)
N1—C11—C12—F121.5 (2)C22—C21—C26—C251.0 (2)
C16—C11—C12—C131.2 (2)N2—C21—C26—C25179.36 (13)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···F160.83 (2)2.30 (2)2.7676 (16)115.8 (17)
N2—H2···F120.86 (2)2.52 (2)3.0784 (17)122.8 (17)
N2—H2···F13i0.86 (2)2.51 (2)3.0949 (19)126.1 (17)
Symmetry code: (i) x, y+2, z.
 

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